AuF3 is reduced in superacidic HF/SbF5 solutions giving three products. 1. Orange [Au3F8 . 2SbF(5)]. It has a layered structure built up by square planar (AuF4)-F-II and (AuF4)-F-III units: Crystal structure: space group P2(1)/c. a = 9.049(2), b = 8.424(1), c = 9.645(1) Angstrom, beta = 115.08(1)degrees. 2. Black [Au3F7 . 3SbF(5)] has a ribbon structure, similarly built up by square planar (AuF4)-F-II and Au(III)F4 units: Crystal structure: space group Pc, a = 9.991(1), b = 10.728(1), c 15.222(1)Angstrom beta = 95.304(2)degrees. 3. Yellow green [(Au(HF)(2)] (SbF6)(2) . 2HF with square planar (AuF4)-F-II units that are formed by two fluorine atoms of the anions and two HF molecules as complex ligands. Crystal structure: Space group P(1) over bar, a = 5.4820) b = 5.8480). c = 9.309(2) Angstrom, alpha = 89.522(4), beta = 85.635(4), gamma = 87.509(4)degrees.